Ni-Mo　alloy　deposit　layer　with　the　amorphous/nanocrystal　microstructure　was　annealed　at　different　heat　temperature　under　the　protection　of　nitrogen.　The　electrochemical　properties　of　the　annealed　Ni-Mo　alloy　coating　were　examined.　The　experamental　result　shows　that　the　amorphous/nanocrystal　Ni-Mo　coatings　have　a　better　hydrogen　evolution　catalytic　activity,　which　depends　on　the　real　contact　area　and　the　amorphous　content　in　the　layer.　When　the　heating　temperature　no　more　than　350°C,　the　deposit　structure　is　still　composed　of　amorphous　phase,　and　the　deposit　exhibits　good　hydrogen　evolution　catalytic　activity.　When　the　temperature　of　heat　treatment　is　higher　than　450°C,　amorphous　content　in　the　deposit　significantly　decreases　and　crystallization　gradually　occurs,　leading　to　a　weaker　hydrogen　evolution　catalytic　activity.